HRID1192042

反应详情

EQUATION

反应方程式

HRID 1192042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 3,4,5-trichloropyridine (1 g, 5.45 mmol) in dichloromethane (20 mL) at 0° C., was added dropwise a 30% hydrogen peroxide solution (1.2 mL, 10.9 mmol). Following the addition, the temperature was allowed to rise to room temperature and was stirred for 15 hours. The reaction mixture was diluted with dichloromethane (50 mL) and was washed with water (10 mL) and then by brine (25 mL×2). The organic phase was dried (Na2SO4), concentrated under vacuum to afford the title product as a white solid (0.8 g, 74% yield). 1H NMR (400 MHz, d6-DMSO) δ: 8.78 (2H, s). MS m/z: 197.90 [M+H]+.

WORKUP

后处理

  1. additionthe addition
  2. customto rise to room temperature
  3. washwas washed with water (10 mL)
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. concentrationconcentrated under vacuum